HRID653410

反应详情

EQUATION

反应方程式

HRID 653410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.43 g of 2,5-dichloropyrimidine was dissolved in 20 mol of dimethyl sulfoxide. To this solution, a mixture of 1.50 g of 4-amino-2-nitrophenol and 5 ml of water, and 2.69 g of potassium carbonate were added, and the mixture was reacted in the atmosphere of nitrogen gas at a temperature of from 100° to 110° C. for 2 hours. After the completion of the reaction, the reaction product was poured into water, and extracted with methylene chloride. The extract layer was washed with brine and dried over anhydrous sodium sulfate, and purified by silica gel column chromatography, whereby 0.74 g of 4-(5-chloro-2-pyrimidinyl)-3-nitroaniline having a melting point of from 151° to 152° C., was obtained.

WORKUP

后处理

  1. additionwere added
  2. customthe mixture was reacted in the atmosphere of nitrogen gas at a temperature of from 100° to 110° C. for 2 hours
  3. customAfter the completion of the reaction
  4. extractionextracted with methylene chloride
  5. washThe extract layer was washed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. custompurified by silica gel column chromatography, whereby 0.74 g of 4-(5-chloro-2-pyrimidinyl)-3-nitroaniline having a melting point of from 151° to 152° C.
  8. customwas obtained